JPS63134662A - Method for synthesizing high hardness boron nitride - Google Patents
Method for synthesizing high hardness boron nitrideInfo
- Publication number
- JPS63134662A JPS63134662A JP27936086A JP27936086A JPS63134662A JP S63134662 A JPS63134662 A JP S63134662A JP 27936086 A JP27936086 A JP 27936086A JP 27936086 A JP27936086 A JP 27936086A JP S63134662 A JPS63134662 A JP S63134662A
- Authority
- JP
- Japan
- Prior art keywords
- boron nitride
- gas
- substrate
- boron
- atoms
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 29
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims description 19
- 230000002194 synthesizing effect Effects 0.000 title claims description 7
- 239000007789 gas Substances 0.000 claims abstract description 33
- 239000000758 substrate Substances 0.000 claims abstract description 26
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 19
- 229910052796 boron Inorganic materials 0.000 claims abstract description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000001257 hydrogen Substances 0.000 claims abstract 2
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 230000005281 excited state Effects 0.000 claims description 2
- 238000001182 laser chemical vapour deposition Methods 0.000 claims description 2
- 239000012495 reaction gas Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 125000004429 atom Chemical group 0.000 abstract description 4
- 239000008246 gaseous mixture Substances 0.000 abstract 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000005520 cutting process Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 5
- 150000004767 nitrides Chemical class 0.000 description 5
- 238000000576 coating method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- -1 iron group metals Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 2
- 229910015844 BCl3 Inorganic materials 0.000 description 1
- 229910015900 BF3 Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
この発明は高硬度な立方晶窒化硼素の合成法に係り、詳
しくは非常に高硬度を有するだけでなく、熱伝導率に富
み、化学的に安定で加えてダイヤモンドとは異なり、鉄
族金属に対する耐性にもすぐれていることから切削工具
、耐摩工具などの工具材料、さらにはヒートシンクなど
の電子材料として用いられる立方晶窒化硼素を気相より
基材表面に析出させる方法に関するものである。[Detailed Description of the Invention] <Industrial Application Field> The present invention relates to a method for synthesizing highly hard cubic boron nitride. Specifically, it not only has very high hardness but also has high thermal conductivity and chemical In addition, unlike diamond, cubic boron nitride is used as tool materials such as cutting tools and wear-resistant tools, as well as electronic materials such as heat sinks because it has excellent resistance to iron group metals. This relates to a method of depositing on the surface of a substrate.
〈従来の技術〉
従来、窒化硼素の製造法としては、
＋１１ １１１ｆ４を含有する蒸発源から基体上に硼素
分子を蒸着させるとともに、少なくとも窒素を含むイオ
ン種を発生せしめるイオン発生源から基体上に該イオン
種を照射して、該基体上に窒化硼素を析出せしめる窒化
ｔＩｌ素膜の製造方法（特公昭６０−１８１２６２号公
報）。<Prior Art> Conventionally, boron nitride has been produced by depositing boron molecules onto a substrate from an evaporation source containing +11 111f4, and depositing boron molecules onto the substrate from an ion source that generates ionic species containing at least nitrogen. A method for producing a nitrided tIl elementary film in which boron nitride is deposited on the substrate by irradiating ion species (Japanese Patent Publication No. 181262/1982).
＋２１ Ｎ２ ＋ Ｎ２プラズマによるＩＩＩ素の化
学輸送を行なうことによって立方晶窒化硼素を生成させ
る方法（Ｊｏｕｒｎａｌ ｏｆ ｌ１ａｔｅｒｉａｌ
５ｃｉｅｎｃｅ １ｅｔｔｅｒｓ ４、（１９８５）
、Ｐ５１〜５４）。+21 Method for producing cubic boron nitride by chemical transport of element III by N2 + N2 plasma (Journal of l1terial
5science 1etters 4, (1985)
, P51-54).
＋３１ ＨＣＤ ｏｕｎで硼素を蒸発させながら、Ｉ
ｌｏｌｌｏｗＡｎｏｄｅからＮ２をイオン化して基板に
放射し、基板には高周波を印加して５ｅｌｆ ｂｉａｓ
効果をもたせて立方晶窒化硼素を生成する方法（Ｐｒｏ
ｃｅｅｄｉｎ９．９ ｔｈ、 ５ｙｎｐｏｓｉｕｎ ｏ
ｎ Ｉｏｎ ５ｏｕｒｃｅ Ｉｏｎ ＡｓｉｓｔｅｄＴ
ｅｃｈｎｏｌｏｇｙ Ａｎｏｄｅ ８５ 、Ｔｏｋｙｏ
（１９８５））。+31 While evaporating boron with HCD own, I
Ionize N2 from the lollowAnode and radiate it to the substrate, apply high frequency to the substrate, and 5elf bias
Method for producing cubic boron nitride with effect (Pro
ceedin9.9th, 5ynposiun o
n Ion 5source Ion AssistedT
technology Anode 85, Tokyo
(1985)).
＋４＋ ｉｌｌ素原子含有固体にＥ８を当てることに
より、硼素を蒸発させ、それに窒素原子含有ガスを流し
こみ、硼素および窒素を同時にイオン化することにより
、基材表面に立方晶窒化硼素を生成する方法（真空、第
２８巻、第７号、１９８５）。+4+ ill A method for producing cubic boron nitride on the surface of a substrate by applying E8 to a solid containing elementary atoms to evaporate boron, and then flowing a nitrogen atom-containing gas into it to simultaneously ionize boron and nitrogen ( Vacuum, Vol. 28, No. 7, 1985).
などが知られている。etc. are known.
〈発明が解決しようとする問題点〉
しかしながら、上記、（１）の方法はイオンビームを発
生する装置および集束装置が高価であることが欠点とさ
れ、（２）の方法は高出力のＲＦプラズマを成膜に利用
していることにより、反応系からの不純物が混入しやす
い。（３）の方法は（１）の方法と同じくイオンビーム
を発生する装置およびその集束装置が高価であることと
、不活性ガスの原子が析出した窒化硼素に取り込まれる
欠点がある。また（４）の方法においては、硼素は融点
と沸点が近いため、Ｅ８を当てることにより、突沸しや
すく制御が困難であるという欠点を有しているのである
。<Problems to be Solved by the Invention> However, the disadvantage of method (1) is that the ion beam generating device and focusing device are expensive, and method (2) requires high-power RF plasma. is used for film formation, impurities from the reaction system are likely to be mixed in. Method (3), like method (1), has the drawbacks that the ion beam generating device and its focusing device are expensive, and that inert gas atoms are incorporated into the precipitated boron nitride. In addition, the method (4) has the disadvantage that since the melting point and boiling point of boron are close to each other, the application of E8 tends to cause bumping and is difficult to control.
く問題点を解決するための手段〉
この発明は上記した従来法の欠点を解消した窒化硼素の
合成法を得るべく検討の結果見出されたものである。Means for Solving the Problems> The present invention was discovered as a result of studies aimed at obtaining a method for synthesizing boron nitride that eliminates the drawbacks of the conventional methods described above.
即ち、この発明は団ｌＡ原子含有ガス、窒素原子含有ガ
スをエキシマレーザ−ＣＶＤ法にて分解、励起状態とし
たのち、高周波プラズマ中を通過せしめることにより３
００〜２０００℃に加熱した基板表面に導入して立方晶
窒化１素を析出させることを特徴とする高硬度窒化硼素
の合成法を提供することを目的とするものである。That is, this invention decomposes a group IA atom-containing gas and a nitrogen atom-containing gas by an excimer laser CVD method, brings them into an excited state, and then passes them through a high-frequency plasma.
The object of the present invention is to provide a method for synthesizing high-hardness boron nitride, which is characterized by introducing cubic mononitride onto the surface of a substrate heated to 00 to 2000°C to precipitate cubic nitride.
く作用〉
この発明においては、硼素原子含有ガスおよび窒素原子
含有ガスの混合ガスをエキシマレーザ−中を通過せしめ
ることにより分解、励起し、励起状の硼素原子および窒
素原子を生成せしめる。かつその励起状の硼素原子およ
び窒素原子をさらに高周波プラズマ中を通過させること
により、より高次のエネルギーを有し、加熱した基板上
において立方晶窒化ｉ木を生成する。Effect> In the present invention, a mixed gas of a boron atom-containing gas and a nitrogen atom-containing gas is passed through an excimer laser to decompose and excite it to generate excited boron atoms and nitrogen atoms. By further passing the excited boron atoms and nitrogen atoms through a high-frequency plasma, cubic nitride i-trees having higher energy are generated on the heated substrate.
このように、この発明においては成膜プロセスとしてエ
キシマレーザ−および高周波プラズマを使用する。Thus, in the present invention, excimer laser and high frequency plasma are used in the film forming process.
上記において、エキシマレーザ−のみ、あるいは高周波
プラズマのみを成膜手段として用いた場合、原料源であ
る硼素原子と窒素原子を互いにｓ ｐ ３結合を行なわ
せるには反応エネルギーが不足するため、非晶質窒化硼
素や六方晶窒化硼素を作成しやすい。In the above, when only an excimer laser or only a high-frequency plasma is used as a film forming means, there is insufficient reaction energy to form sp 3 bonds between boron atoms and nitrogen atoms, which are the raw material sources, so the amorphous It is easy to create pure boron nitride and hexagonal boron nitride.
これに対して、エキシマレーザ−と高周波プラズマの２
つの成膜手段を組合せて利用した場合、硼素原子と窒素
原子が互いにｓ ｐ ３結合を起こすのに充分な反応エ
ネルギーが得られるのである。On the other hand, excimer laser and high frequency plasma
When these two film forming methods are used in combination, sufficient reaction energy can be obtained to cause sp 3 bonds between boron atoms and nitrogen atoms.
上記においてエキシマレーザ−出力は１〜１００Ｗの範
囲が好適である。これは１Ｗより小さいと、成膜速度が
非常に小さくなり、かつ原料源を励起するのに不足し、
また１００Ｗより大きいと、媒質ガスの寿命が短くなる
ため、出力減衰が顕著となり、安定した出力を得ること
はできない。In the above, the excimer laser output is preferably in the range of 1 to 100W. If this is less than 1W, the film formation rate will be very low and it will be insufficient to excite the raw material source.
Moreover, if it is larger than 100 W, the lifetime of the medium gas will be shortened, resulting in significant output attenuation, making it impossible to obtain stable output.
次に高周波プラズマの出ツノは１００ｗ以上が好ましい
。これは１００Ｗより小さいと、励起硼素原子と励起窒
素原子を互いにｓ ｐ３結合を行なわせるにはエネルギ
ーが不足するためである。Next, it is preferable that the output power of the high-frequency plasma is 100 W or more. This is because if the power is less than 100 W, there is insufficient energy to cause the excited boron atoms and the excited nitrogen atoms to form sp3 bonds with each other.
基板温度は３００℃より低いと、励起状態の硼素原子と
窒素原子が互いにｓ ｐ ３結合する熱エネルギーとし
て不足し、また２０００℃より高くなると、成膜する窒
化硼素膜から窒素が抜は出てしまうため、３００〜２０
００℃が好ましい。If the substrate temperature is lower than 300°C, there is insufficient thermal energy for the excited boron atoms and nitrogen atoms to bond with each other sp3, and if it is higher than 2000°C, nitrogen is extracted from the boron nitride film being formed. 300~20 to store
00°C is preferred.
この発明において、使用するエキシマレーザ−の媒質ガ
スとしてはＡｒＦ、 ￥−ｒＦ、Ｆ２ガスなどが用い
られる。In this invention, ArF, \-rF, F2 gas, etc. are used as the medium gas of the excimer laser.
硼素原子含有ガス中の硼素原子数および窒素原子含有ガ
ス中の窒素原子数の比はＢ／Ｎ＝ ０．１〜１０の範囲
が好ましい。これはＢ／Ｎ＜０．１の時は非晶質状の窒
化硼素の膜が析出されやすく、Ｂ／Ｎ〉１００時は硼素
が過剰となり、非晶質状の硼素が形成されやすいためで
ある。The ratio of the number of boron atoms in the boron atom-containing gas to the number of nitrogen atoms in the nitrogen atom-containing gas is preferably in the range of B/N=0.1 to 10. This is because when B/N<0.1, an amorphous boron nitride film tends to be deposited, and when B/N>100, boron becomes excessive and amorphous boron is likely to be formed. be.
硼素原子含有ガスとしてＢ２ＨいＢＣｌ３、ＢＢｒ＊、
Ｂ、Ｎ、Ｈ６などが挙げられ、窒素原子含有ガスとじて
はＮ２、Ｎ ８３等が用いられる。As a boron atom-containing gas, B2H, BCl3, BBr*,
Examples include B, N, H6, etc., and N2, N83, etc. are used as the nitrogen atom-containing gas.
なおこの発明で高硬度窒化硼素合成に際しては、第１図
あるいは第２図に概略図として示す製造装置を使用する
。そして第１図は基板をヒーターにて加熱するタイプで
あり、第２図は高周波プラズマ中に基板が位置している
のでプラズマ強度によって基板温度を調節できるタイプ
である。In the present invention, when synthesizing high hardness boron nitride, a manufacturing apparatus shown schematically in FIG. 1 or 2 is used. FIG. 1 shows a type in which the substrate is heated with a heater, and FIG. 2 shows a type in which the substrate is placed in high-frequency plasma, so that the substrate temperature can be adjusted depending on the plasma intensity.
両図におりて、１は硼素原子含有ガス供給装置、２は窒
素原子含有ガス供給装置、３はエキシマレーザ−発生装
置、４は反応室、５はエキシマレーザ−ガイド、６はエ
キシマレーザ−１７は基板、８は基板支持台、９はヒー
ター、１０は高周波コイル、１１は高周波電源、１２は
コック、１３は排気装置、１４は排気口である。In both figures, 1 is a boron atom-containing gas supply device, 2 is a nitrogen atom-containing gas supply device, 3 is an excimer laser generator, 4 is a reaction chamber, 5 is an excimer laser guide, and 6 is an excimer laser 17 1 is a substrate, 8 is a substrate support stand, 9 is a heater, 10 is a high frequency coil, 11 is a high frequency power source, 12 is a cock, 13 is an exhaust device, and 14 is an exhaust port.
〈実施例〉 以下実施例によりこの発明の詳細な説明する。<Example> The present invention will be explained in detail below with reference to Examples.
実施例１
第１図に示す製造装置を用い、シリコンウェハーを基板
として使用し、原料ガスとしてジボランおよび窒素を夫
々２０ｃｃ／ｌ１ｉｎ、 １０ｃｃ／ｍ１ｎｔした。Example 1 A manufacturing apparatus shown in FIG. 1 was used, a silicon wafer was used as a substrate, and diborane and nitrogen were used as source gases at 20 cc/l1in and 10 cc/mlnt, respectively.
反応管内圧力は０． ＩＴｏｒｒに調整し、基板温度を
９００℃とした。エキシマレーザ−としてＡｒ Ｆレー
ザーを使用し、レーザー出力は２０ｗとした。高周波周
波数は１３．５６ Ｍ ｌ−１ｚ 、高周波出力は５０
０Ｗとし、成膜時間は４時間とした。The pressure inside the reaction tube is 0. It was adjusted to ITorr, and the substrate temperature was 900°C. An Ar F laser was used as the excimer laser, and the laser output was 20W. High frequency frequency is 13.56 M l-1z, high frequency output is 50
The power was 0W, and the film forming time was 4 hours.
成膜終了後、６μ而面度の窒化硼′ｉＡ膜が析出され、
Ｘ１１回折で評価したところ、２０ ＝ ４３．２度付
近に鋭いピークを検出し、立方晶窒化硼素であると固定
した。After the film formation was completed, a 6 μm thick boron nitride film was deposited.
When evaluated by X11 diffraction, a sharp peak was detected near 20 = 43.2 degrees, and it was determined that it was cubic boron nitride.
実施例２
第２図に示す製造装置を用い、シリコンウェハーを基板
として使用し、原料ガスとして塩化硼素、窒素を夫々８
ｃｃ／ｎｔｎ、 １６ｃｃ／ｎ１ｎｉした。Example 2 Using the manufacturing apparatus shown in Fig. 2, a silicon wafer was used as the substrate, and boron chloride and nitrogen were each used as raw material gases.
cc/ntn, 16cc/n1ni.
反応管内圧力は０．３Ｔｏｒｒに調整し、基板温度を１
１００℃とした。エキシマレーザ−としてに、Ｆレーザ
ーを使用し、レーザー出力は３０ｗとした。高周波周波
数は１３．５６ Ｍ ＨＺ 、高周波出力は１ｋｗとし
、成膜時間は７時間とした。The pressure inside the reaction tube was adjusted to 0.3 Torr, and the substrate temperature was adjusted to 1.
The temperature was 100°C. An F laser was used as the excimer laser, and the laser output was 30W. The high frequency frequency was 13.56 MHz, the high frequency output was 1 kW, and the film forming time was 7 hours.
成膜終了後、１２μｍ程度の窒化硼Ｘ膜が析出され、ラ
マン分析で評価したところ１３１０ｃ、−１と１０５５
ｃＪ＋−１付近に鋭いピークを検出し、立方晶窒化硼素
と同定できた。After the film formation was completed, a 12 μm thick boron nitride
A sharp peak was detected near cJ+-1, and it was identified as cubic boron nitride.
実施例３ 第１図に示す製造装置を使用した。Example 3 A manufacturing apparatus shown in FIG. 1 was used.
モリブデンを基板として用い、原料ガスとしてフッ化硼
素、アンモニアを夫々１０ｃｃ／１ｎ、 ３０ｃｃ／１
ｎ流した。反応管内圧力は０．２Ｔｏｒｒに調整し、基
板温度を８００℃とした。成膜手段としてエキシマレー
ザ−は使用せず、高周波プラズマのみとし、高周波周波
数１３．５６ Ｍ ＨＺ 、高周波出力を４００ｗとし
、成膜時間を５時間とした。Using molybdenum as a substrate, boron fluoride and ammonia were used as source gases at 10cc/1n and 30cc/1, respectively.
n flowed. The pressure inside the reaction tube was adjusted to 0.2 Torr, and the substrate temperature was 800°C. Excimer laser was not used as a film forming means, only high frequency plasma was used, the high frequency frequency was 13.56 MHz, the high frequency output was 400 W, and the film forming time was 5 hours.
成膜修了後、５μ乳程度の窒化硼素膜が析出され、Ｘ８
回折で評価したところ、２θ＝ ２６．７度および４３
．２度付近に夫々広いピークを検出し、六方晶窒化ｌＩ
Ｉ素および立方晶窒化ｉｓの混在した薄膜であることが
認められた。After the film formation is completed, a boron nitride film of about 5 μm is deposited, and
As evaluated by diffraction, 2θ = 26.7 degrees and 43
．． Broad peaks were detected around 2 degrees, and hexagonal nitride lI
It was confirmed that the film was a mixture of I element and cubic crystal nitride IS.
実施例４
上記実施例１〜３の条件を用いてＷＣＣ超超硬合金ある
ＴＮＭＧ４３２をチップとして用いて該チップ上にコー
ティングを行ない、切削テストを行なりた。Example 4 Using the conditions of Examples 1 to 3 above, a WCC cemented carbide, TNMG432, was used as a chip, a coating was applied on the chip, and a cutting test was conducted.
比較としてコーティングを行なわないチップおよびＣＶ
Ｉ）法にてＴ、Ｎコーティングを行なったチップの切削
テストをも行なった。Chip and CV without coating for comparison
A cutting test was also conducted on chips coated with T and N using the method I).
コーティングは何れも被覆層厚３μｍとした。All coatings had a coating layer thickness of 3 μm.
切削テスト条件は第１表に示した。また切削テストの結
果は第２表に示した。The cutting test conditions are shown in Table 1. The results of the cutting test are shown in Table 2.
第 １ 表
第 ２ 表
上表から立方晶窒化硼素を被覆層としてチップに使用し
た場合、この発明の実施例は全て耐摩耗性にすぐれてい
ることが認められた。From Table 1 and Table 2, it was found that all the examples of the present invention had excellent wear resistance when cubic boron nitride was used as a coating layer in the chip.
また、この発明で得たＣＢＮコートチップの鋼旋削にお
ける切削性能を切削速度と寿命時間との関係で調べたと
ころ第３図の結果を得、さらに鋳鉄切削における欠損ま
での切削時間と衝撃回数との関係を調べたところ第４図
の結果を得た。Furthermore, the cutting performance of the CBN-coated insert obtained in this invention in steel turning was investigated in terms of the relationship between cutting speed and life time, and the results shown in Figure 3 were obtained. When we investigated the relationship, we obtained the results shown in Figure 4.
〈発明の効果〉
以上説明したように、この発明は耐熱衝撃性、熱伝導性
、硬度、耐摩耗性および高温における鉄族金属に対する
耐性にもすぐれる立方品窒化硼素膿を気相から析出する
新規な合成法であり、切削部材、耐摩耗部材および耐熱
部品の被覆膜として用いた場合、第２図および第３図に
示すように多大な効果を示すことが認められた。<Effects of the Invention> As explained above, the present invention precipitates cubic boron nitride pus from the gas phase, which has excellent thermal shock resistance, thermal conductivity, hardness, wear resistance, and resistance to iron group metals at high temperatures. This is a novel synthesis method, and when used as a coating film for cutting members, wear-resistant members, and heat-resistant parts, it has been found to have great effects as shown in FIGS. 2 and 3.
第１図および第２図はこの発明の方法にて用いる製造装
置の概略説明図、第３図および第４図はこの発明の方法
で得られる立方晶窒化ｌ１１素を被覆膜としたチップの
切削性能を示す図表である。
１・・・硼素原子含有ガス供給装置
２・・・窒素原子含有ガス供給装置
３・・・エキシマレーザ−発生装置
４・・・反応室 ６・・・エキシマレーザ−
７・・・基板 ９・・・ヒーター１０・・
・高周波コイル １１・・・高周波電源出願人代理
人 弁理士 和 １）昭第１図
第３図
第２図
第４＠Figures 1 and 2 are schematic explanatory diagrams of the manufacturing equipment used in the method of the present invention, and Figures 3 and 4 show chips coated with cubic l11 element nitride obtained by the method of the present invention. It is a chart showing cutting performance. 1... Boron atom-containing gas supply device 2... Nitrogen atom-containing gas supply device 3... Excimer laser generator 4... Reaction chamber 6... Excimer laser
7... Board 9... Heater 10...
・High frequency coil 11... High frequency power supply applicant's agent Patent attorney Kazu 1) Showa 1, 3, 2, 4 @
Claims (2)
シマレーザーＣＶＤ法にて分解、励起状態としたのち、
高周波プラズマ中を通過せしめることにより３００〜２
０００℃に加熱した基板表面に導入し、立方晶窒化硼素
を析出させることを特徴とする高硬度窒化硼素の合成法
。(1) After decomposing a boron atom-containing gas and a nitrogen atom-containing gas by excimer laser CVD method and bringing them into an excited state,
300~2 by passing through high frequency plasma.
A method for synthesizing high-hardness boron nitride, which is characterized by introducing cubic boron nitride onto the surface of a substrate heated to 000°C to precipitate cubic boron nitride.
ガス中の窒素原子数との比較をＢ／Ｎ＝０．１〜１０の
範囲として反応ガスに水素を用いない特許請求の範囲第
１項記載の高硬度窒化硼素の合成法。(2) A claim in which the number of boron atoms in the boron atom-containing gas and the number of nitrogen atoms in the nitrogen atom-containing gas are in the range of B/N = 0.1 to 10 and hydrogen is not used as the reaction gas. A method for synthesizing high hardness boron nitride according to item 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61279360A JPH0819523B2 (en) | 1986-11-22 | 1986-11-22 | High hardness boron nitride synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61279360A JPH0819523B2 (en) | 1986-11-22 | 1986-11-22 | High hardness boron nitride synthesis method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63134662A true JPS63134662A (en) | 1988-06-07 |
| JPH0819523B2 JPH0819523B2 (en) | 1996-02-28 |
Family
ID=17610080
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61279360A Expired - Lifetime JPH0819523B2 (en) | 1986-11-22 | 1986-11-22 | High hardness boron nitride synthesis method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0819523B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0263549A (en) * | 1988-08-27 | 1990-03-02 | Agency Of Ind Science & Technol | Process and apparatus for plasma reaction |
| US5463901A (en) * | 1991-09-27 | 1995-11-07 | Sumitomo Electric Industries, Ltd. | Stacked piezoelectric surface acoustic wave device with a boron nitride layer in the stack |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6063372A (en) * | 1983-09-19 | 1985-04-11 | Agency Of Ind Science & Technol | Manufacture of thin boron nitride film of high hardness |
| JPS6184379A (en) * | 1984-09-29 | 1986-04-28 | Kyocera Corp | Production of high-hardness boron nitride film |
| JPS61224318A (en) * | 1985-03-29 | 1986-10-06 | Hitachi Ltd | Device and method for formation of vapor-phase thin film |
-
1986
- 1986-11-22 JP JP61279360A patent/JPH0819523B2/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6063372A (en) * | 1983-09-19 | 1985-04-11 | Agency Of Ind Science & Technol | Manufacture of thin boron nitride film of high hardness |
| JPS6184379A (en) * | 1984-09-29 | 1986-04-28 | Kyocera Corp | Production of high-hardness boron nitride film |
| JPS61224318A (en) * | 1985-03-29 | 1986-10-06 | Hitachi Ltd | Device and method for formation of vapor-phase thin film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0263549A (en) * | 1988-08-27 | 1990-03-02 | Agency Of Ind Science & Technol | Process and apparatus for plasma reaction |
| US5463901A (en) * | 1991-09-27 | 1995-11-07 | Sumitomo Electric Industries, Ltd. | Stacked piezoelectric surface acoustic wave device with a boron nitride layer in the stack |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0819523B2 (en) | 1996-02-28 |
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